3-[(MethylaMino)Methyl]-benzaMide HCl synthesis

Yield:956234-96-1 57%

Reaction Conditions:

with potassium hydroxide in isopropyl alcohol; for 2 h;Heating / reflux;

Steps:

50

To a solution of 7.98 g (54.6 mmol) of Intermediate 49 in 80 ml of isopropanol, 7.98 g (142.2 mmol) of powdered KOH (85%) were added. The mixture was stirred for 2 hours at reflux temperature. The solvent was reduced under reduced pressure. The obtained residue was dissolved in a small volume of water and extracted several times with dichloromethane. The organic extracts were combined, dried (MgSO₄), and concentrated. The residue was treated with hexane and concentrated (x3). The obtained residue was treated with chloroform and concentrated (x3), and finally the residual solvents were eliminated using an oil vacuum pump. The title compound was obtained as an oil that slowly solidified at room temperature. (5.14 g, 57%).

References:

WO2007/124898,2007,A1 Location in patent:Page/Page column 45